CN105675809A - Analysis method of concentration of HI-I2-H2O ternary solution - Google Patents
Analysis method of concentration of HI-I2-H2O ternary solution Download PDFInfo
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- CN105675809A CN105675809A CN201610029128.XA CN201610029128A CN105675809A CN 105675809 A CN105675809 A CN 105675809A CN 201610029128 A CN201610029128 A CN 201610029128A CN 105675809 A CN105675809 A CN 105675809A
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Abstract
The invention provides an analysis method of concentration of an HI-I2-H2O ternary solution, and belongs to the field of chemical analysis technology. Firstly, mathematical relationship between concentration of HI-I2-H2O ternary solution standard samples and density of materials is established, mathematical relationship between concentration and viscosity is established, and a system of simultaneous equations is formed; density and viscosity of the HI-I2-H2O ternary solution to be measured with unknown concentration are respectively determined by using a density testing apparatus and a viscosity apparatus, and concrete concentration of the sample to be measured is solved by using the equation set. The method has high accuracy degree; when an on-line densitometer and a viscometer are used, on-line and real time determination of concentration of the HI-I2-H2O ternary solution is realized; the defects of a conventional chemical titration analysis method, such as sampling danger, complex operation, process time consumption without online testing, and the like are overcome.
Description
Technical field
The present invention relates to a kind of containing iodine hydroiodic acid (i.e. hydrogen iodide-iodo-water ternary solution, HI-I2-H2O) concentration analysis, belongs to chemical analysis technology field.
Background technology
Containing iodine hydroiodic acid feed liquid (i.e. hydrogen iodide-iodo-water ternary solution, HI-I2-H2O) component analysis operation, in the analysis of routine experimentation room, heat chemistry iodine-sulfur process hydrogen production by water decomposition technique, and all can use in hydroiodic acid production technology. For heat chemistry iodine-sulfur process hydrogen production by water decomposition technique, in iodine-sulfur process hydrogen production process, the hydroiodic acid relying on Bunsen reaction to generate, owing to adding excessive iodine, define HI-I2-H2O thing phase, determines HI-I exactly2-H2The concentration of each component in O, the research to related process, so that the control of site technique flow process is all extremely important.
Conventional HI-I2-H2O concentration analysis is titrimetry, determines the concentration of HI specifically with acid-base titrations, and with sodium thiosulfate solution titrated method, namely iodimetric titration determines I2Concentration, so can obtain HI-I2-H2Concrete component and content (remaining component, i.e. a H in O2The content of O then can be drawn by MaterialBalance Computation). Although titrimetry has the advantages such as amount of samples is few, but due to I in material2Existence, the accuracy of titrimetry is relatively difficult to ensure card, this is because electricity is to I2/I-Normal potential neither high not low yet, I2Can as oxidant by strong reducing agent reduce, iodide ion also can as reducing agent by strong or strong oxidant aoxidize, therefore titration process is disturbed by the factor such as the acid-base value of material to be measured, oxygen in air, repeatability is poor, and titrimetry needs volumetric solution used carried out preparation, Accurate Calibration and rationally preserve in advance, gratifying result can be obtained, therefore there is the defect that complex operation, process are consuming time.
And additionally it is important that HI-I2-H2O has stronger volatility and strong corrosivity, particularly heating, pressurization operating condition under. Well imagine, this liquid material be very difficult in the pipeline of actual production line, container with sampling, analyze. Due to above reason, it is necessary to for HI-I2-H2O finds more particularly suitable concentration analysis.
By Gibbs phase rule it can be seen that when thermodynamical equilibrium, the relation between the number of components of system, the number of phases and number of degrees of freedom, is: F=C-P+2
In formula: the number of degrees of freedom, of F-system;The number of components of C-system; P-is the number of phase in selected system;
Wherein number of degrees of freedom, F is when system is poised state, in the number situation not changing phase, and the number of the factor (independent variable, such as temperature, pressure, density etc.) that can independently change, and for HI-I2-H2This three compositions system of O, at normal pressure with under fixed temperature,
F=C (3 kinds of components)-P (1 phase)+0 (constant temperature normal pressure, this entry value is 0)=2
Number of degrees of freedom, F is 2, it was shown that as long as determining HI-I2-H22 factors that can independently change (i.e. independent variable) of O system, all physico-chemical properties of this system are and determine value (naturally including its composition and concentration). Therefore, optional 2 independent variables being relatively easy to gather, determine HI-I by them2-H2The concentration data of O sample. At HI-I2-H2In the physicochemical properties that O solution is numerous, density and viscosity the two variable are separate, simultaneously all closely related with the composition of solution again, as HI or I in solution2Content when changing, the density of solution and viscosity can significantly change. Therefore, density, viscosity can determine HI-I as independent variable2-H2The concentration of O.
HI-I2-H2The density of O material and viscosity number are the parameters being easier to measure, it can be measured by the method and the instrument that have multiple maturation, such as density value, the gentle graduated cylinder weighing method in sky can be adopted simply to measure, also float type densimeter, density bottle, U-tube oscillatory type densimeter can be used to measure, and this can also have multiple on-line checking means, such as gamma-ray densitometer, online density transmitter etc., or after adopting the pressure reduction of one group of determination of pressure sensor certain altitude difference material, calculate density value. And viscosity number can adopt rotary viscosimeter, ultrasonic type viscometer or capillary viscosimeter to be measured, wherein contain a variety of online viscosimeter, particularly ultrasonic activation formula in-line viscometer equally.
HI-I2-H2The density of O material, concentration are two mutual independences physical quantitys closely-related with solution composition again, it is prone to detect the characteristic being even capable of on-line checking simultaneously, enables us to determine the HI-I at setting pressure and temperature by mensuration density, concentration the two variable2-H2The concentration of O material, its theoretical foundation as previously mentioned: to HI-I under fixed temperature, pressure condition2-H2The number of degrees of freedom, of O system is 2. And for HI-I2-H2The characteristic of this liquid material of O, the change of temperature on its density, viscosity has comparatively significantly affects, and when the general technology of 0.1 to 10MPa, its volume (i.e. density) is affected only small by pressure, viscosity influence is also less, therefore when carrying out density, viscosity test, main consideration temperature conditions.
Be can be seen that by above analysis, it is possible to by measuring density, concentration the two variable determines the HI-I at setting pressure and temperature2-H2The concentration of O material.
Summary of the invention
It is an object of the invention to provide a kind of analysis method containing iodine hydriodic acid concentration, namely by the method for founding mathematical models, replace conventional chemical titration assay method, it is to avoid its sampling danger, complex operation, process be consuming time, cannot the shortcoming such as on-line checking.
Technical scheme is as follows:
A kind of analysis method containing iodine hydriodic acid concentration, it is characterised in that the method comprises the steps:
1) prepare a series of have gradient concentration distribution containing iodine hydroiodic acid standard sample;
2) density measuring device is adopted to measure each standard sample density value at the same temperature;
3) viscosimeter is adopted to measure each standard sample viscosity number under above-mentioned same temperature;
4) by Mathematical Fitting, set up containing the relationship between the concentration of iodine hydroiodic acid, density and viscosity three:
ρ=a1+b1·x+c1·y(1)
η=a2+b2·x+c2·y+d2·x2+e2·y2+f·x·y(2)
In formula: ρ is the density value containing iodine hydroiodic acid, unit is g/mL;
η is the viscosity number containing iodine hydroiodic acid, and unit is centipoise;
X represents the concentration of HI in material, and unit is mol/L;
Y represents I2Concentration, unit is mol/L;
a1、b1、c1、a2、b2、c2、d2、e2It is the parameter value obtained in Mathematical Fitting process with f;
5) adopting density measuring device to determine the density value containing iodine hydroiodic acid sample to be measured, when during mensuration, the temperature of material is with bioassay standard sample rate, the temperature of material is consistent; Adopting viscosimeter to determine the viscosity number containing iodine hydroiodic acid sample to be measured, when during mensuration, the temperature of material is with bioassay standard sample rate, the temperature of material is consistent;
6) utilize step 4) in formula (1) and (2) simultaneous calculate the concentration containing iodine hydroiodic acid sample to be measured.
Density measuring device of the present invention adopts balance-graduated cylinder, float type densimeter, density bottle, U-tube oscillatory type densimeter, gamma-ray densitometer, online density transmitter or pressure transducer.
Viscosimeter of the present invention adopts rotary viscosimeter, ultrasonic type viscometer or capillary viscosimeter.
The present invention has the following advantages and salience effect: due to the fact that employing density value and viscosity number are as location parameter, data acquisition is convenient and swift, analysis result is accurate, can overcome conventional titration analyze method complex operation, process consuming time, cannot the shortcoming such as on-line checking; And need not prepare and use any chemical reagent and chemical analysis instrument.
Detailed description of the invention
Below in conjunction with embodiment, the detailed description of the invention of the analysis method containing iodine hydriodic acid concentration of the present invention is described in further details. These embodiments are merely to illustrate the present invention, and are not limitation of the present invention.
The analysis method containing iodine hydriodic acid concentration that the present invention proposes, it specifically includes following steps:
1) prepare a series of have gradient concentration distribution containing iodine hydroiodic acid standard sample;
2) adopting density measuring device to measure each standard sample density value at the same temperature, density measuring device can adopt the gentle graduated cylinder in sky, float type densimeter, density bottle, U-tube oscillatory type densimeter, gamma-ray densitometer, online density transmitter or pressure transducer etc.;
3) adopting viscosimeter to measure each standard sample viscosity number under above-mentioned same temperature, viscosimeter can adopt rotary viscosimeter, ultrasonic type viscometer or capillary viscosimeter etc.;
4) by Mathematical Fitting, set up containing the relationship between the concentration of iodine hydroiodic acid, density and viscosity three:
ρ=a1+b1·x+c1·y(1)
η=a2+b2·x+c2·y+d2·x2+e2·y2+f·x·y(2)
In formula: ρ is the density value containing iodine hydroiodic acid, unit is g/mL;
η is the viscosity number containing iodine hydroiodic acid, and unit is centipoise (cP);
X represents the concentration of HI in material, and unit is mol/L;
Y represents I2Concentration, unit is mol/L;
a1、b1、c1、a2、b2、c2、d2、e2It is the parameter value obtained in Mathematical Fitting process with f;
5) adopting density measuring device to determine the density value containing iodine hydroiodic acid sample to be measured, when during mensuration, the temperature of material is with bioassay standard sample rate, the temperature of material is consistent; Adopting viscosimeter to determine the viscosity number containing iodine hydroiodic acid sample to be measured, when during mensuration, the temperature of material is with bioassay standard sample rate, the temperature of material is consistent;
6) utilize step 4) in formula (1) and (2) simultaneous calculate the concentration containing iodine hydroiodic acid sample to be measured.
Under computer software is assisted, utilizing the formula (1) obtained under different temperatures and (2) to be fitted, the density containing iodine hydroiodic acid and the viscosity that record under available arbitrary temp are calculated, and draw its concentration information.
Embodiment 1
Preparation HI:I2: H2The molar ratio of O be a series of variable concentrations in the scope of 1:0.2～4.0:4.0～13 containing iodine hydroiodic acid standard sample.
Anton Paar DMA4100M type U-tube oscillatory type densimeter is adopted to measure each standard sample density value under normal pressure, 80 DEG C of conditions respectively;
In atmospheric conditions, the viscosity number at the above-mentioned each standard sample of determination of ubbelohde viscometer 80 DEG C is utilized.
By the concentration value of each standard sample obtained, density value, viscosity number carries out Mathematical Fitting, obtains its relationship and is:
ρ=0.9718+0.09110x+0.1917y (1)
η=0.8568-0.1979x-0.0810y+0.02328x2+0.01469y2x+0.03213xy(2)
In formula: ρ is the density value containing iodine hydroiodic acid, unit is g/mL;
η is the viscosity number containing iodine hydroiodic acid, and unit is centipoise (cP);
X represents the concentration of HI in material, and unit is mol/L;
Y represents I2Concentration, unit is mol/L;
According to above-mentioned relation formula, once obtain ρ and η value, the value of x, y can be calculated, also just can calculate HI, I2Concentration, and the concentration of H2O can obtain via mass balance.
As shown in the following chart, 1#, 2# and the 3# hydroiodic acid sample containing iodine to be measured is carried out concentration analysis, identical with above-mentioned standard sample, same measure normal pressure, density value at 80 DEG C with Anton Paar DMA4100M type U-tube oscillatory type densimeter, and with its viscosity number at 80 DEG C of determination of ubbelohde viscometer. The equation group utilizing (1), (2) to constitute, solves the concentration information obtaining sample. As a comparison, table also list the concentration of 1#, 2# and 3# sample adopting conventional titration method to obtain.
Embodiment 2:
As shown in the following chart, to 4#With 5#The hydroiodic acid sample containing iodine to be measured carries out concentration analysis, at ambient pressure, is placed in the tantalum storage tank of a 1.5L by the hydroiodic acid sample containing iodine that volume is 1L, and the temperature controlling storage pot liquid is 80 DEG C. This storage tank is equipped with gamma-ray densitometer and ultrasonic type in-line viscometer, and the density they determined, concentration values substitute into the equation group that embodiment one is obtained, solves the concentration information obtained containing iodine hydroiodic acid sample. As a comparison, table also list adopt conventional titration method to obtain 4#With 5#The concentration of number sample.
Embodiment 3:
Adopt in embodiment one configure containing iodine hydroiodic acid standard sample, adopt Anton Paar DMA4100M type U-tube oscillatory type densimeter and Ubbelohde viscometer, measure each standard sample density value under 10,20,30,40,50,60,70,80,90,100,110 and 120 DEG C of temperature conditions and viscosity number at ambient pressure respectively. Obtain the CONCENTRATION DENSITY-viscosity relation under series of temperature.
Above-mentioned series relational expression is loaded a computer, matching can be interpolated under software is assisted, utilize what record under different temperature points to extrapolate its concentration information containing the density of iodine hydroiodic acid, viscosity.
As shown in the following chart, to 6#With 7#The hydroiodic acid sample containing iodine to be measured carries out concentration analysis, and under 1Mpa, volume is the 6 of 1.1L#Or 7#The hydroiodic acid sample containing iodine is placed in the tantalum pressing pressure storage tank of a 1.5L, and the temperature controlling storage pot liquid is 95 DEG C. This storage tank is equipped with gamma-ray densitometer and ultrasonic type in-line viscometer, and density, viscosity signal that these instruments collect are received row number of going forward side by side and process by above computer, calculate the concentration information containing iodine hydroiodic acid sample.
Claims (3)
1. the analysis method containing iodine hydriodic acid concentration, it is characterised in that the method comprises the steps:
1) prepare a series of have gradient concentration distribution containing iodine hydroiodic acid standard sample;
2) density measuring device is adopted to measure each standard sample density value at the same temperature;
3) viscosimeter is adopted to measure each standard sample viscosity number under above-mentioned same temperature;
4) by Mathematical Fitting, set up containing the relationship between the concentration of iodine hydroiodic acid, density and viscosity three:
ρ=a1+b1·x+c1·y(1)
η=a2+b2·x+c2·y+d2·x2+e2·y2+f·x·y(2)
In formula: ρ is the density value containing iodine hydroiodic acid, unit is g/mL;
η is the viscosity number containing iodine hydroiodic acid, and unit is centipoise;
X represents the concentration of HI in material, and unit is mol/L;
Y represents I2Concentration, unit is mol/L;
a1、b1、c1、a2、b2、c2、d2、e2It is the parameter value obtained in Mathematical Fitting process with f;
5) adopting density measuring device to determine the density value containing iodine hydroiodic acid sample to be measured, when during mensuration, the temperature of material is with bioassay standard sample rate, the temperature of material is consistent; Adopting viscosimeter to determine the viscosity number containing iodine hydroiodic acid sample to be measured, when during mensuration, the temperature of material is with bioassay standard sample rate, the temperature of material is consistent;
6) utilize step 4) in formula (1) and (2) simultaneous calculate the concentration containing iodine hydroiodic acid sample to be measured.
2. a kind of analysis method containing iodine hydriodic acid concentration according to claim 1, it is characterised in that: described density measuring device adopts balance-graduated cylinder, float type densimeter, density bottle, U-tube oscillatory type densimeter, gamma-ray densitometer, online density transmitter or pressure transducer.
3. a kind of analysis method containing iodine hydriodic acid concentration according to claim 1, it is characterised in that: described viscosimeter adopts rotary viscosimeter, ultrasonic type viscometer or capillary viscosimeter.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108152343A (en) * | 2017-11-14 | 2018-06-12 | 清华大学 | The analytical equipment and method of a kind of hydriodic acid concentration containing iodine |
| CN110514555A (en) * | 2018-05-22 | 2019-11-29 | 泰科电子(上海)有限公司 | Concentration detection apparatus, concentration measurement and control device and solar water heater |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108152343A (en) * | 2017-11-14 | 2018-06-12 | 清华大学 | The analytical equipment and method of a kind of hydriodic acid concentration containing iodine |
| CN108152343B (en) * | 2017-11-14 | 2020-01-17 | 清华大学 | Iodine-containing hydriodic acid concentration analysis equipment and method |
| CN110514555A (en) * | 2018-05-22 | 2019-11-29 | 泰科电子(上海)有限公司 | Concentration detection apparatus, concentration measurement and control device and solar water heater |
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